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CAS No. : | 16874-34-3 | MDL No. : | MFCD08063871 |
Formula : | C7H12O3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | GQQLWKZRORYGHY-UHFFFAOYSA-N |
M.W : | 144.17 | Pubchem ID : | 10103286 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrazine; In butan-1-ol; for 3h;Heating / reflux; | a) (rac.)-(Tetrahydro-furan-2-yl)-acetic acid hydrazide A solution of (rac.)-(tetrahydro-furan-2-yl)-acetic acid ethyl ester (3.84 g, 24 mmol) in n-butanol (24 mL) was treated with hydrazine hydrate (1.4 mL, 29 mmol) and the resulting mixture was then heated under reflux for 3 h. The solvent was evaporated and residual volatile components were azeotropically removed by coevaporation with toluene. Chromatographic purification (SiO2, dichloromethane:methanol:aq.ammonia (25%)=100:0:0 to 90:10:1) afforded the title compound as a viscous, colorless oil (1.1 g, 32%). 1H-NMR (300 MHz, DMSO): delta=1.45 (mc, 1H), 1.70-1.95 (m, 3H), 2.13 (dd, J=6 Hz, J=14 Hz, 1H), 2.24 (dd, J=7 Hz, J=14 Hz, 1H), 3.56 (dd, J=8 Hz, J=14 Hz, 1H), 3.72 (dd, J=7 Hz, J=14 Hz, 1H), 4.05 (mc, 1H), 4.16 (s, 2H), 8.94 (s, 1H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
96.9% | With 5%-palladium/activated carbon; hydrogen; In ethanol; at 30 - 150℃; under 15001.5 Torr;Large scale; | 10359] 3010 g (21.5 mol) of thran-2-carboxylic acid ethyl ester, 500 ml of ethanol (1% MEK) and 20 g of catalyst, palladium on A-carbon dry, 5% Pd, type K-0227T) are initially introduced together and heated under a hydrogen pressure of 20 bat The reaction starts at 30-40C. and is relatively strongly exothermic. After 1-1.5 hat 60-70 C., the hydrogen absorption is as good as finished. The mixture is slowly heated to 140-150 C. and then stirred for a further 2-3 hat this temperature. GC control: starting material no longer present.10360] Filter off from the catalyst and concentrate the filtrate on a rotary evaporator (water bath: 60-70 C., 200-20 mbar). The crude yield is 3055 g.10361] The evaporated crude product is distilled with the addition of 0.1% by weight of Na2CO3 over a short column (b.p.: 9 1-93 C./40 mbar).10362] Yield: 2999 g (96.9% of theory)10363] ?H NMR (400 MHz, chioroform-d) oe 4.44 (dd, J=8.4, 5.2 Hz, 1H), 4.20 (qd, J=7.1, 1.7 Hz, 2H), 4.05-3.98 (m, 1H), 3.95-3.88 (m, 1H), 2.30-2.19 (m, 1H), 2.06-1.85 (m, 3H), 1.29 (t, J=7.1 Hz, 3H)10364] ?3C NMR (101 MHz, CDC13) oe 173.38, 76.80,69.33, 60.87, 30.20, 25.27, 14.24 |
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